CN101799407A - Method for measuring content of halogen - Google Patents
Method for measuring content of halogen Download PDFInfo
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- CN101799407A CN101799407A CN 201010136751 CN201010136751A CN101799407A CN 101799407 A CN101799407 A CN 101799407A CN 201010136751 CN201010136751 CN 201010136751 CN 201010136751 A CN201010136751 A CN 201010136751A CN 101799407 A CN101799407 A CN 101799407A
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- oxygen bomb
- absorption liquid
- oxygen
- iodide
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Abstract
The invention relates to the field of analysis and testing, in particular to a method for measuring the content of halogen. Requirements on the accuracy of measuring the content of the chlorine ions and the content of the bromonium ions in products become higher and higher along with the constant deepening of non-halogenated requirements on industrial products. In the process of measuring the content of chlorine and the content of bromine in products, the invention makes improvement on the stage of processing a sample by the oxygen bomb combustion method, adding iodine ions into the existing absorption liquid so as to convert silver chloride precipitation and silver bromide precipitation into silver iodide precipitation, thereby enabling that the chlorine ions and the bromonium ions are free, facilitating the rear measurement of the chlorine content and the bromine content in products by utilizing ion chromatograph, and increasing the accuracy of detection.
Description
Technical field
The invention belongs to the analytical test field, specifically be meant the assay method of content of halogen.
Background technology
Along with deepening continuously of the non-halogen requirement of industry, requirement for the accuracy of test of chloride in the product, bromine is also more and more higher, present detection method all adopts standard EN 14582:2007 to carry out sample preparation, carry out quantitative test with ion chromatograph then, sample treatment is described below in the standard: sample (calorimetric bomb that contains high pressure oxygen) in airtight system is oxidized by burning, compound chloride, bromine is separately converted to chloride, bromide is absorbed solution then and absorbs and/or be dissolved in the absorbent solution.
Because absorption liquid is Na
2CO
3/ NaHCO
3Blend absorbent, so can only be with the dissolving of soluble chlorine, bromine thing, and can not be with insoluble chlorine, the dissolving of bromine thing, thereby, carry out causing in the test of quantitative analysis test inaccurate at next step ion chromatograph.
In view of testing standard EN 14582 to " in initial sample, exist or can not measure fully by the method at insoluble halogenide, bromide that combustion step produces." description, some detection companies to the mensuration of this type of material by adopting: earlier sample is carried out organic solvent extractionprocess and extracts processing, adopt the method for EN 14582 that clear liquid is partly carried out sample test then, and with this test result as conclusion.But may contain the halogen-containing material that is insoluble to this extraction organic solvent in these samples, thereby cause testing deviation.
Summary of the invention
The objective of the invention is to: at the deficiency that exists in the existing method of testing, provide a kind of reasonably, the method for testing of chlorine, bromide ion content fast and accurately.
The present invention improved the stage of oxygen bomb burn processing sample, in existing absorption liquid, add iodide ion, can make silver chloride, silver bromide precipitation be converted to the silver iodide precipitation, thereby make chlorine, bromide ion dissociate out, be convenient to the rear portion ion chromatograph and test, increase the accuracy that detects.
Concrete steps in the technical solution of the present invention are elaborated as follows:
Sample preparation:
1, claims sample: take by weighing sample 0.1～1g (being accurate to 0.0001g) to the oxygen bomb sample cup, in cup, add the conventional combustion adjuvant of 0.3～0.6ml then, but the total amount of sample and combustion adjuvant must not surpass 1.5g.
2, dress ignition wire and sample: open the oxygen bomb lid, the sample cup that fills sample is fixed, the ignition wire two ends of an appropriate length are fixed on the electrode column, and it is contacted with sample and do not contact sample cup;
3, add absorption liquid:
A) preparation of absorption liquid: Na in the absorption liquid
2CO
3Concentration is 0.5～2.2mmol/l, NaHCO
3Concentration is 0.5～2.5mmol/l, and solubility iodate substrate concentration is 10～50mmol/l, fully mixes, and makes to contain the iodide absorption liquid.Wherein solubility iodate thing comprises sodium iodide and potassium iodide.Preferably, Na in the absorption liquid
2CO
3Concentration is 0.8～2.0mmol/l, NaHCO
3Concentration is 0.8～2.2mmol/l, and solubility iodate substrate concentration is 20～40mmol/l, fully mixes, and makes to contain the iodide absorption liquid.
B) interpolation of absorption liquid: in the oxygen bomb cup, add 10～20ml and contain the iodide absorption liquid, make oxygen bomb cup inwall wetting, with on the oxygen bomb bowl cover and tighten;
4, oxygenation: oxygen catheter is connected on the oxygen bomb bowl cover, slowly charge into oxygen, start from scratch the compartment of terrain increasing until 1～1.5MPa, stop 3～5s, discharge the air in the oxygen bomb then lentamente, behind the triplicate again oxygenation to oxygen gauge be shown as 2.5～3.0MPa and end, stop 3～5s, the combustion-supporting gas during as burning;
5, igniting: connect harness, closed circuit is lighted sample, finishes after the sample combustion heat release to the oxygen bomb;
6, cooling and vibration: oxygen bomb is put into cooling bath, make the height of water be in about 2/3 place of oxygen bomb body and be advisable.About 15～20min treats to place it in the 20～30min that vibrates up and down on the oscillator after the oxygen bomb cooling, and institute's measured ion is absorbed by liquid absorption fully;
7, venting: take off oxygen bomb, slowly bleed off the oxygen of the inside with air release;
8, filtration and constant volume: the absorption liquid filtration is transferred in the volumetric flask of 100mL, more than 3 times, is transferred in the volumetric flask, use the deionized water constant volume again with proper amount of deionized water drip washing oxygen bomb cylinder, sample cup and oxygen bomb lid;
Sample test:
1, standard curve making: measure a certain amount of standard solution from containing having the card standard solution of 1000mg/l, dilute each leading element solution gradually, the working solution that will contain every kind of element 5 μ g, 10 μ g, 20 μ g, 30 μ g, 40 μ g, 50 μ g moves into constant volume in the volumetric flask of 100mL, makes calibration curve.Adopt ion chromatograph to carry out quantitatively the standard solution after the dilution, measure the absorption intensity peak area reading of object element, set up the calibration curve of object element absorption intensity and concentration relationship with calibration curve.
2, specimen: after setting up calibration curve, test laboratory reagent blank and sample solution, the same calibration curve of integral way.If select sample solution concentration to exceed the concentration range of calibration curve, should be diluted in the respective alignment curve concentration range after test again again.
Na is only arranged in the absorption liquid of original technology
2CO
3Or NaHCO
3, do not have solubility iodate thing.
Advantage of the present invention and good effect are: add the iodide that contain iodide ion in the absorption liquid of original technology, can make silver chloride, silver bromide precipitation be converted to the silver iodide precipitation, thereby make chlorine, bromide ion dissociate out, loss does not make test result more near actual value.
Test specification: chlorine, bromine content are greater than 50mg/kg.
Embodiment
The invention will be further described below by specific embodiment, but embodiment of the present invention are not limit so.
Embodiment 1
The sample preparation stage:
1, claims sample: take by weighing sample 1g (being accurate to 0.0001g) to the oxygen bomb sample cup, in cup, add the conventional combustion adjuvant of 0.6ml then, but the total amount of sample and combustion adjuvant must not surpass 1.5g.
2, dress ignition wire and sample: open the oxygen bomb lid, the sample cup that fills sample is fixed, the ignition wire two ends of an appropriate length are fixed on the electrode column, and it is contacted with sample and do not contact sample cup;
3, add absorption liquid:
A) preparation of absorption liquid: Na in the absorption liquid
2CO
3Concentration is 0.8mmol/l, NaHCO
3Concentration is 1.5mmol/l, and the concentration of sodium iodide is 20mmol/l, fully mixes, and makes to contain the iodide absorption liquid.
B) interpolation of absorption liquid: in the oxygen bomb cup, add 15ml and contain the iodide absorption liquid, make oxygen bomb cup inwall wetting, with on the oxygen bomb bowl cover and tighten;
4, oxygenation: oxygen catheter is connected on the oxygen bomb bowl cover, slowly charge into oxygen, start from scratch the compartment of terrain increasing until 1.5MPa, stop 3s, discharge the air in the oxygen bomb then lentamente, behind the triplicate again oxygenation to oxygen gauge be shown as 2.5-3.0MPa and end, stop 5s, the combustion-supporting gas during as burning;
5, igniting: connect harness, closed circuit is lighted sample, finishes after the sample combustion heat release to the oxygen bomb;
6, cooling and vibration: oxygen bomb is put into cooling bath, make the height of water be in about 2/3 place of oxygen bomb body and be advisable.Behind about 15min, treat to place it in the 25min that vibrates up and down on the oscillator after the oxygen bomb cooling, institute's measured ion is absorbed by liquid absorption fully;
7, venting: take off oxygen bomb, slowly bleed off the oxygen of the inside with air release;
8, filtration and constant volume: the absorption liquid filtration is transferred in the volumetric flask of 100mL, more than 3 times, is transferred in the volumetric flask, use the deionized water constant volume again with proper amount of deionized water drip washing oxygen bomb cylinder, sample cup and oxygen bomb lid.
The sample test stage:
1, standard curve making: measure a certain amount of standard solution from containing having the card standard solution of 1000mg/l, dilute each leading element solution gradually, the working solution that will contain every kind of element 5 μ g, 10 μ g, 20 μ g, 30 μ g, 40 μ g, 50 μ g moves into constant volume in the volumetric flask of 100mL, makes calibration curve.Adopt ion chromatograph to carry out quantitatively the standard solution after the dilution, measure the absorption intensity peak area reading of object element, set up the calibration curve of object element absorption intensity and concentration relationship with calibration curve.
2, specimen: after setting up calibration curve, test laboratory reagent blank and sample solution, the same calibration curve of integral way.If select sample solution concentration to exceed the concentration range of calibration curve, should be diluted in the respective alignment curve concentration range after test again again.
Embodiment 2
The sample preparation stage:
1, claims sample: take by weighing sample 0.8g (being accurate to 0.0001g) to the oxygen bomb sample cup, in cup, add the conventional combustion adjuvant of 0.3ml then, but the total amount of sample and combustion adjuvant must not surpass 1.5g.
2, dress ignition wire and sample: open the oxygen bomb lid, the sample cup that fills sample is fixed, the ignition wire two ends of an appropriate length are fixed on the electrode column, and it is contacted with sample and do not contact sample cup;
3, add absorption liquid:
A) preparation of absorption liquid: Na in the absorption liquid
2CO
3Concentration is 1.0mmol/l, NaHCO
3Concentration is 2.0mmol/l, and the concentration of potassium iodide is 30mmol/l, fully mixes, and makes to contain the iodide absorption liquid.
B) interpolation of absorption liquid: in the oxygen bomb cup, add 18ml and contain the iodide absorption liquid, make oxygen bomb cup inwall wetting, with on the oxygen bomb bowl cover and tighten;
4, oxygenation: oxygen catheter is connected on the oxygen bomb bowl cover, slowly charge into oxygen, start from scratch the compartment of terrain increasing until 1.0MPa, stop 4s, discharge the air in the oxygen bomb then lentamente, behind the triplicate again oxygenation to oxygen gauge be shown as 2.5-3.0MPa and end, stop 3s, the combustion-supporting gas during as burning;
5, igniting: connect harness, closed circuit is lighted sample, finishes after the sample combustion heat release to the oxygen bomb;
6, cooling and vibration: oxygen bomb is put into cooling bath, make the height of water be in about 2/3 place of oxygen bomb body and be advisable.Behind the 20min, treat to place it in the 30min that vibrates up and down on the oscillator after the oxygen bomb cooling, institute's measured ion is absorbed by liquid absorption fully;
7, venting: take off oxygen bomb, slowly bleed off the oxygen of the inside with air release;
8, filtration and constant volume: the absorption liquid filtration is transferred in the volumetric flask of 100mL, more than 3 times, is transferred in the volumetric flask, use the deionized water constant volume again with proper amount of deionized water drip washing oxygen bomb cylinder, sample cup and oxygen bomb lid;
Sample test:
1, standard curve making: measure a certain amount of standard solution from containing having the card standard solution of 1000mg/l, dilute each leading element solution gradually, the working solution that will contain every kind of element 5 μ g, 10 μ g, 20 μ g, 30 μ g, 40 μ g, 50 μ g moves into constant volume in the volumetric flask of 100mL, makes calibration curve.Adopt ion chromatograph to carry out quantitatively the standard solution after the dilution, measure the absorption intensity peak area reading of object element, set up the calibration curve of object element absorption intensity and concentration relationship with calibration curve.
2, specimen: after setting up calibration curve, test laboratory reagent blank and sample solution, the same calibration curve of integral way.If select sample solution concentration to exceed the concentration range of calibration curve, should be diluted in the respective alignment curve concentration range after test again again.
Claims (5)
1. method for measuring content of halogen, comprise sample preparation stage and mensuration stage, the sample preparation stage comprises again: claim sample, dress ignition wire and sample, add absorption liquid, oxygenation, igniting, cooling and vibration, venting, filtration and constant volume totally eight steps, it is characterized in that: in adding in the absorption liquid step of sample preparation stage, in absorption liquid, add solubility iodate thing, make and contain the iodide absorption liquid.
2. a kind of method for measuring content of halogen according to claim 1 is characterized in that: described solubility iodate thing is sodium iodide, potassium iodide.
3. a kind of method for measuring content of halogen according to claim 1 is characterized in that: described consisting of of iodide absorption liquid: the Na that contains
2CO
30.5～2.2mmol/l, NaHCO
30.5～2.5mmol/l, solubility iodate thing 10～50mmol/l fully mixes, and makes to contain the iodide absorption liquid.
4. a kind of method for measuring content of halogen according to claim 1 is characterized in that: described consisting of of iodide absorption liquid: the Na that contains
2CO
30.8～2.0mmol/l, NaHCO
30.8～2.2mmol/l, solubility iodate thing 20～40mmol/l fully mixes, and makes to contain the iodide absorption liquid.
5. a kind of method for measuring content of halogen according to claim 1, it is characterized in that: determination step is as follows:
Sample preparation:
A) claim sample: take by weighing sample 0.1～1g (being accurate to 0.0001g) to the oxygen bomb sample cup, in cup, add the conventional combustion adjuvant of 0.3～0.6ml then, but the total amount of sample and combustion adjuvant must not surpass 1.5g;
B) dress ignition wire and sample: open the oxygen bomb lid, the sample cup that fills sample is fixed, the ignition wire two ends are fixed on the electrode column, and it is contacted with sample and do not contact sample cup;
C) add absorption liquid: in the oxygen bomb cup, add 10～20ml and contain the iodide absorption liquid, make oxygen bomb cup inwall wetting, with on the oxygen bomb bowl cover and tighten;
D) oxygenation: oxygen catheter is connected on the oxygen bomb bowl cover, slowly charge into oxygen, start from scratch the compartment of terrain increasing until 1～1.5MPa, stop 3～5s, discharge the air in the oxygen bomb then lentamente, behind the triplicate again oxygenation to oxygen gauge be shown as 2.5～3.0MPa and end, stop 3～5s, the combustion-supporting gas during as burning;
E) igniting: connect harness, closed circuit is lighted sample, finishes after the sample combustion heat release to the oxygen bomb;
F) cooling and vibration: oxygen bomb is put into cooling bath, make the height of water be in the 15～20min of about 2/3 place of oxygen bomb body, treat to place it in the 20～30min that vibrates up and down on the oscillator after the oxygen bomb cooling, institute's measured ion is absorbed by liquid absorption fully;
G) venting: take off oxygen bomb, slowly bleed off the oxygen of the inside with air release;
H) filtration and constant volume: the absorption liquid filtration is transferred in the volumetric flask of 100mL, more than 3 times, is transferred in the volumetric flask, use the deionized water constant volume again with deionized water drip washing oxygen bomb cylinder, sample cup and oxygen bomb lid;
Sample test:
A. standard curve making: measure a certain amount of standard solution from containing having the card standard solution of 1000mg/l, dilute each leading element solution gradually, the working solution that will contain every kind of element 5 μ g, 10 μ g, 20 μ g, 30 μ g, 40 μ g, 50 μ g moves into constant volume in the volumetric flask of 100mL, make calibration curve, adopt ion chromatograph to carry out quantitatively the standard solution after the dilution, measure the absorption intensity peak area reading of object element, set up the calibration curve of object element absorption intensity and concentration relationship with calibration curve;
B. sample test: after setting up calibration curve, test laboratory reagent blank and sample solution, the same calibration curve of integral way is selected sample solution concentration, if exceed the concentration range of calibration curve, will be diluted in the respective alignment curve concentration range.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101367518A CN101799407B (en) | 2010-03-26 | 2010-03-26 | Method for measuring content of halogen |
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|---|---|---|---|
| CN2010101367518A CN101799407B (en) | 2010-03-26 | 2010-03-26 | Method for measuring content of halogen |
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| CN101799407B CN101799407B (en) | 2012-04-25 |
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|---|---|---|---|
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102706949A (en) * | 2012-05-24 | 2012-10-03 | 清华大学 | Method for determination of inorganic element in fuel gas |
| CN102818780A (en) * | 2012-08-13 | 2012-12-12 | 瓮福（集团）有限责任公司 | Rapid determination method for bromine in oil-gas field water |
| CN102928400A (en) * | 2012-10-15 | 2013-02-13 | 深圳市谱尼测试科技有限公司 | Method for measuring content of heavy metal in polymer |
| CN105973666A (en) * | 2016-05-04 | 2016-09-28 | 新奥科技发展有限公司 | Chlorine and sulfur extraction and determination method and apparatus thereof |
| CN106018666A (en) * | 2016-06-24 | 2016-10-12 | 苏州新区环保服务中心有限公司 | Oxygen bomb combustion method for testing content of halogens and content of sulphur in industrial solid waste |
| CN106198776A (en) * | 2016-06-22 | 2016-12-07 | 江西瑞林稀贵金属科技有限公司 | Measure the method for halogen in waste and old circuit board smelting smoke dust |
| CN106526030A (en) * | 2016-12-08 | 2017-03-22 | 大连百傲化学股份有限公司 | Analysis method of bromine content in industrial liquid chlorine |
| CN108362814A (en) * | 2017-12-31 | 2018-08-03 | 浙江易测环境科技有限公司 | A kind of adsorbable organic halogen detection method |
| CN108663405A (en) * | 2018-06-19 | 2018-10-16 | 湖南师范大学 | A kind of Oxygen Bomb Combustion quickly measures the detection method of chlorine content in coal |
| CN108802149A (en) * | 2018-06-19 | 2018-11-13 | 湖南师范大学 | A kind of Oxygen Bomb Combustion quickly measures the detection method of PAHs in coal content |
| CN109030703A (en) * | 2018-06-08 | 2018-12-18 | 江苏省产品质量监督检验研究院 | A kind of method of content of halogen in Oxygen Bomb Combustion-sulfate by ion chromatography cable nonmetallic materials |
| CN110133173A (en) * | 2018-02-02 | 2019-08-16 | 佛山市华祥检测技术服务有限公司 | Measuring method for chlorine in fiberboard and bromo element content |
| CN110398564A (en) * | 2019-06-24 | 2019-11-01 | 广东省特种设备检测研究院中山检测院 | The detection method of chlorinity in a kind of solid biomass fuel |
| CN111413421A (en) * | 2020-02-20 | 2020-07-14 | 广东电科院能源技术有限责任公司 | Method for testing content of chloride ions in dust after sludge combustion and control method |
| CN112557142A (en) * | 2020-12-24 | 2021-03-26 | 广州博诺通技术股份有限公司 | Sample pretreatment method, halogen content detection method and application |
| CN113777254A (en) * | 2021-04-27 | 2021-12-10 | 浙江信汇新材料股份有限公司 | Method for measuring halogen in water |
| CN114994235A (en) * | 2022-06-23 | 2022-09-02 | 浙江微通催化新材料有限公司 | Application of oxygen bomb combustion method in determination of palladium-carbon-chlorine content and determination method |
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| CN102706949A (en) * | 2012-05-24 | 2012-10-03 | 清华大学 | Method for determination of inorganic element in fuel gas |
| CN102818780A (en) * | 2012-08-13 | 2012-12-12 | 瓮福（集团）有限责任公司 | Rapid determination method for bromine in oil-gas field water |
| CN102928400A (en) * | 2012-10-15 | 2013-02-13 | 深圳市谱尼测试科技有限公司 | Method for measuring content of heavy metal in polymer |
| CN105973666A (en) * | 2016-05-04 | 2016-09-28 | 新奥科技发展有限公司 | Chlorine and sulfur extraction and determination method and apparatus thereof |
| CN106198776A (en) * | 2016-06-22 | 2016-12-07 | 江西瑞林稀贵金属科技有限公司 | Measure the method for halogen in waste and old circuit board smelting smoke dust |
| CN106198776B (en) * | 2016-06-22 | 2019-04-26 | 中国瑞林工程技术股份有限公司 | The method for measuring halogen in waste and old circuit board smelting smoke dust |
| CN106018666A (en) * | 2016-06-24 | 2016-10-12 | 苏州新区环保服务中心有限公司 | Oxygen bomb combustion method for testing content of halogens and content of sulphur in industrial solid waste |
| CN106018666B (en) * | 2016-06-24 | 2017-12-22 | 苏州新区环保服务中心有限公司 | The method of halogen and sulfur content in oxygen bomb combustion measure industrial solid castoff |
| CN106526030A (en) * | 2016-12-08 | 2017-03-22 | 大连百傲化学股份有限公司 | Analysis method of bromine content in industrial liquid chlorine |
| CN106526030B (en) * | 2016-12-08 | 2019-01-11 | 大连百傲化学股份有限公司 | It is a kind of industry liquid chlorine in bromine content analysis method |
| CN108362814A (en) * | 2017-12-31 | 2018-08-03 | 浙江易测环境科技有限公司 | A kind of adsorbable organic halogen detection method |
| CN110133173A (en) * | 2018-02-02 | 2019-08-16 | 佛山市华祥检测技术服务有限公司 | Measuring method for chlorine in fiberboard and bromo element content |
| CN109030703A (en) * | 2018-06-08 | 2018-12-18 | 江苏省产品质量监督检验研究院 | A kind of method of content of halogen in Oxygen Bomb Combustion-sulfate by ion chromatography cable nonmetallic materials |
| CN108802149A (en) * | 2018-06-19 | 2018-11-13 | 湖南师范大学 | A kind of Oxygen Bomb Combustion quickly measures the detection method of PAHs in coal content |
| CN108663405A (en) * | 2018-06-19 | 2018-10-16 | 湖南师范大学 | A kind of Oxygen Bomb Combustion quickly measures the detection method of chlorine content in coal |
| CN110398564A (en) * | 2019-06-24 | 2019-11-01 | 广东省特种设备检测研究院中山检测院 | The detection method of chlorinity in a kind of solid biomass fuel |
| CN111413421A (en) * | 2020-02-20 | 2020-07-14 | 广东电科院能源技术有限责任公司 | Method for testing content of chloride ions in dust after sludge combustion and control method |
| CN112557142A (en) * | 2020-12-24 | 2021-03-26 | 广州博诺通技术股份有限公司 | Sample pretreatment method, halogen content detection method and application |
| CN112557142B (en) * | 2020-12-24 | 2024-05-31 | 广州博诺通技术股份有限公司 | Sample pretreatment method, halogen content detection method and application |
| CN113777254A (en) * | 2021-04-27 | 2021-12-10 | 浙江信汇新材料股份有限公司 | Method for measuring halogen in water |
| CN114994235A (en) * | 2022-06-23 | 2022-09-02 | 浙江微通催化新材料有限公司 | Application of oxygen bomb combustion method in determination of palladium-carbon-chlorine content and determination method |
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|---|---|
| CN101799407B (en) | 2012-04-25 |
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